CN112763635A - Gas chromatographic column, application and low-boiling-point fluorine-containing compound separation method - Google Patents
Gas chromatographic column, application and low-boiling-point fluorine-containing compound separation method Download PDFInfo
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Abstract
The invention belongs to the technical field of chemical analysis and detection, and particularly discloses a gas chromatographic column, application of the gas chromatographic column and a method for separating low-boiling-point fluorine-containing compounds by using the gas chromatographic column. The gas chromatographic column provided by the invention can realize good chromatographic separation efficiency at room temperature by selecting a mode of connecting the silica carrier packed column and the PTFE micro powder carrier packed column in series and coating the fixed liquid of the polytrifluorochloroethylene oil, and can also protect the carrier from being oxidized, thereby greatly prolonging the service time of the chromatographic column. Experiments prove that the low-boiling-point fluorine-containing compound is separated by adopting the gas chromatographic column and adopting a low-temperature constant-temperature separation and medium-flow-rate method, the gas chromatographic column has the advantages of high column efficiency, good selectivity and high analysis speed, and the separation peak is clearer when the gas chromatographic column is used for separating the low-boiling-point fluorine-containing compound.
Description
Technical Field
The invention relates to the technical field of chemical analysis and detection, in particular to a gas chromatographic column, application thereof and a method for separating low-boiling-point fluorine-containing compounds by adopting the gas chromatographic column.
Background
In the production process of fluorine-containing fine chemicals, various active intermediates and byproducts with various properties or corrosiveness are easily generated due to the strong oxidizing property of fluorine atoms, and a large amount of fluorine-containing substances with boiling points lower than 0 ℃ exist, so that the separation and accurate quantitative analysis of the fluorine-containing compounds are the key for ensuring the stable development of production.
Currently, chemical analysis and chromatographic analysis are mostly adopted for monitoring and analyzing raw materials, intermediates and byproducts. In chemical analysis methods, the methods adopted in large quantity are gravimetric analysis and titrimetric analysis, and the substance content is calculated by means of color change, precipitation generation, weight increase and decrease, enrichment, masking and the like, so that the analysis method has large errors and cannot be applied to multi-component analysis. Therefore, simultaneous chromatography is required. Chromatographic analysis, also known as chromatography, utilizes the selective distribution of different substances in different phase states to elute a mixture in a mobile phase versus a stationary phase, and the substances in the mixture move along the stationary phase at different speeds, thereby achieving the separation purpose. The chromatographic analysis method has the advantages of high efficiency, rapidness, small sample consumption and the like, and is widely applied to the process control and monitoring of chemical production.
Particularly to the production of fluorine-containing chemicals, in the production process, a part of raw materials, intermediates and byproducts are contained in a reaction system, and simultaneously, the reaction system has low boiling point, strong oxidizing property and corrosive components, such as F2、COF2、CF3OF, etc., which have extremely low boiling points OF less than-70 ℃ and are liable to react with the carrier and the fixing liquid, resulting in failure OF the column. Experiments find that the existing capillary column and the conventional packed chromatographic column are difficult to achieveEfficient separation and accurate quantification of low boiling components. Therefore, it is necessary to study the separation technique of low boiling point fluorine-containing compounds to find a method for performing effective separation analysis of low boiling point fluorine-containing compounds.
Disclosure of Invention
The invention mainly solves the technical problem of providing a gas chromatographic column which is specially used for separating and analyzing low-boiling-point fluorine-containing compounds and has good chromatographic separation efficiency.
The invention also provides a method for separating the low-boiling-point fluorine-containing compound by adopting the gas chromatographic column, and the chromatographic column has clear separation peak and high column efficiency when being used for separating the low-boiling-point fluorine-containing compound.
In order to solve the technical problems, the invention adopts a technical scheme that: the utility model provides a gas chromatographic column, is including the first packed column and the second packed column that concatenate, pack the microballon silica gel carrier of coating polytrifluorochloroethylene in the first packed column, pack the PTFE miropowder carrier of coating polytrifluorochloroethylene in the second packed column. By selecting a mode of serially connecting a silica carrier packed column and a PTFE micro powder carrier packed column and coating polytrifluorochloroethylene, good chromatographic separation efficiency at room temperature can be realized, the carrier can be protected from being oxidized, and the service life of the chromatographic column is greatly prolonged.
As a preferred technical scheme, the microsphere silica gel carrier coated with the polychlorotrifluoroethylene is prepared by impregnating the microsphere silica gel carrier with polychlorotrifluoroethylene oil, and the mass ratio of the microsphere silica gel carrier to the polychlorotrifluoroethylene oil is (8-10) to 1.
According to a preferable technical scheme, the PTFE micro powder carrier coated with the polytrifluorochloroethylene is prepared by impregnating and coating polytrifluorochloroethylene oil on the PTFE micro powder carrier, and the mass ratio of the PTFE micro powder carrier to the polytrifluorochloroethylene oil is (4-6) to 1. According to the characteristics of the separated low-boiling-point fluorine-containing compound, the separation efficiency of the chromatogram can be improved and the separation effect is better by setting the filling carrier in the first filling column and the second filling column and the coated polytrifluorochloroethylene oil to different mass ratios.
Preferably, the microThe particle size of the microsphere silica gel carrier is 80-100 meshes, and/or the specific surface area of the microsphere silica gel carrier is more than or equal to 250m2(ii)/g; the particle size of the PTFE micro powder carrier is 80-100 meshes. By selecting the carrier with specific particle size, the column efficiency of the chromatographic column can be improved, the selectivity is enhanced, and the purpose of improving the separation effect is achieved.
Preferably, the column length ratio of the first packed column to the second packed column is (4-6) to 3.
Preferably, the first packed column is a stainless steel column and the second packed column is a PTFE column.
As a further preferred embodiment, the column length of the first packed column is 5m, and the column length of the second packed column is 3 m; the inner diameters of the first packed column and the second packed column are both 1.5 mm.
The gas chromatographic column provided by the invention is a gas chromatographic column special for separating and analyzing low-boiling-point fluorine-containing compounds, and can be applied to separating and/or analyzing samples containing low-boiling-point fluorine-containing compounds, wherein the low-boiling-point fluorine-containing compounds are optionally selected from C2F4、F2、CF4、CF3OF、COF2And CF3One or more of COFs.
When the separation is detected, the opening of the first packed column is a sample inlet end and is used for being connected with a sample inlet of a gas chromatograph, and the opening of the second packed column is a detector end and is used for being connected with a detector.
The invention also provides a method for separating low-boiling-point fluorine-containing compounds by adopting the gas chromatographic column, which comprises the following steps:
(1) connecting an opening of the first packed column with a sample inlet of a gas chromatograph, and connecting an opening of the second packed column with a detector; helium is used as carrier gas, the pressure of the carrier gas is 0.05-0.15 MPa, the flow rate of the carrier gas is set to be 20-30 ml/min, the temperature of a column box is increased from room temperature to 75-85 ℃ at the temperature increase rate of 4-6K/min, the temperature is kept, the aging is carried out, and then the temperature is reduced to the sample measuring temperature;
(2) after the base line is observed to be stable, the sample injection temperature is set to be 95-105 ℃, the temperature of the column incubator is set to be constant at 25-35 ℃, the temperature of the detector is set to be 75-85 ℃, and then the sample to be detected is injected and enters the sample injection systemLine separation detection; the sample to be detected is a sample containing the low-boiling-point fluorine-containing compound, and the low-boiling-point fluorine-containing compound is optionally selected from C2F4、F2、CF4、CF3OF、COF2And CF3One or more of COFs.
Experiments prove that when the chromatographic column is used for separating the low-boiling-point fluorine-containing compound, the separation peak is clearer and the column efficiency is higher.
The gas chromatographic column provided by the invention is prepared by connecting a first filling column and a second filling column in series, wherein a microsphere silica gel carrier coated with a fixing solution is filled in the first filling column, a PTFE micro powder carrier coated with the fixing solution is filled in the second filling column, and the used fixing solution is polychlorotrifluoroethylene oil. The first packing column and the second packing column select different stationary phases, the first packing column mainly realizes effective separation of components with extremely low boiling point (lower than minus 30 ℃) and molecular weight less than 170 in the low-boiling-point fluorine-containing compound, and the second packing column mainly realizes effective separation of components with medium high boiling point and large molecular weight and modifies chromatographic peak shape. The separation effect of the chromatographic column depends on the selected stationary phase, the operation condition and the like, and the invention adopts a mode of serially connecting a silica carrier packed column and a PTFE micro powder carrier packed column and then coats the fixed liquid polychlorotrifluoroethylene oil, thereby realizing good chromatographic separation efficiency at room temperature, protecting the carrier from being oxidized and greatly prolonging the service time of the chromatographic column. Experiments prove that the low-boiling-point fluorine-containing compound is separated by adopting the gas chromatographic column and adopting a low-temperature constant-temperature separation and medium-flow-rate method, the gas chromatographic column has the advantages of high column efficiency, good selectivity and high analysis speed, and the separation peak is clearer when the gas chromatographic column is used for separating the low-boiling-point fluorine-containing compound.
Drawings
FIG. 1 is a gas chromatogram obtained in example 2 of the present invention;
FIG. 2 is a gas chromatogram obtained in comparative example 1 of the present invention.
Detailed Description
The technical solution of the present invention will be explained in detail below.
Aiming at the technical problem in the analysis of the existing fluorine-containing fine chemicals, the invention provides a gas chromatographic column special for the separation and analysis of low-boiling-point fluorine-containing compounds. Specifically, the general gas chromatographic column for analyzing the fluorine-containing micromolecule compounds is formed by connecting two filling columns, wherein the first filling column can adopt a stainless steel column with the outer diameter of 3mm, the inner diameter of 1.5mm and the length of 5m as a column body, and the carrier selects 80-100 meshes and/or the specific surface area is more than or equal to 250m2For the microsphere silica gel, the fixing solution was polychlorotrifluoroethylene oil (Kel-F oil). The second packed column can be PTFE (polytetrafluoroethylene) column with outer diameter of 3mm, inner diameter of 1.5mm and length of 3m, the carrier is PTFE micropowder for chromatography of 80-100 meshes, and the stationary liquid is polychlorotrifluoroethylene oil (Kel-F oil).
Before preparing the gas chromatography column, the column and the packed carrier need to be treated:
firstly, the first packed column and the second packed column are cleaned before use, and the cleaning method comprises the following steps: sequentially washing twice with hot alkali solution and weak acid solution, continuously washing with 500ml deionized water, and drying the column for later use;
secondly, the microsphere silica gel carrier for the first packed column is processed at high temperature before use, and the processing method comprises the following steps: measuring a certain volume of microspherical silica gel, placing the microspherical silica gel in a big beaker, drying the microspherical silica gel in an oven at 200 ℃ for 24 hours, taking out the microspherical silica gel and cooling the microspherical silica gel to room temperature for later use; drying the second packed column with PTFE micropowder carrier under infrared lamp for 10min, cooling, and storing in a dryer for use.
The following provides a preparation method of a gas chromatographic column, which comprises the following steps:
s1: accurately measuring 17.7ml of microsphere silica gel, weighing the microsphere silica gel and calculating the weight as a1Weighing the fixed liquid polychlorotrifluoroethylene oil by the weight of a2，a2＝0.1a10.9, placing the stationary liquid in a beaker, adding 20ml of acetone, and stirring until the acetone is completely dissolved to obtain a stationary liquid solution; then, adding the microsphere silica gel into the fixing solution while stirring the fixing solution, and then placing under an infrared lamp until the solvent is completely evaporated;
s2: accurately measuring 13.9ml of PTFE fine powder, weighing the powder and calculating the weight as b1Weighing the fixed liquid polychlorotrifluoroethylene oil by the weight of b2，b2＝0.18b10.82, adding 11ml of acetone into the stationary liquid, and stirring until the acetone is completely dissolved to obtain a stationary liquid solution; then, stirring the stationary liquid solution while adding PTFE micro powder into the stationary liquid solution, then placing under an infrared lamp until the solvent is completely evaporated, wherein the PTFE micro powder is easy to agglomerate, and the dried powder is sieved by a 100-mesh stainless steel sieve under the infrared lamp to ensure the particle size of the filler;
s3: filling the carrier coated with the stationary liquid prepared in the step S1 into a first filling column by adopting a decompression method, wherein the filling column is required to be tapped continuously to ensure that the carrier is uniformly distributed in the filling process, and after filling, the column head is plugged by glass wool, so that the first filling column is prepared;
filling the carrier coated with the stationary liquid prepared in the step S2 into a second filling column by adopting a decompression method, wherein the filling column is required to be tapped continuously to ensure that the carrier is uniformly distributed in the filling process, and whether the carrier is tightly filled is observed under light, after filling, a column head is plugged by glass wool, and the second filling column is prepared;
and (3) placing a stainless steel liner tube with the diameter of 1.5mm into the column head of the second packed column, and connecting the first packed column and the second packed column in series by using a stainless steel nut to prepare the gas chromatographic column.
The method for separating and detecting the low-boiling-point fluorine-containing compound by adopting the gas chromatographic column comprises the following steps:
s1: the filling inlet of the gas chromatographic column is marked as a gas inlet, and the other end of the filling inlet is an outlet; setting the flow rate of carrier gas to be 20-30 ml/min, connecting the opening of the first packed column with the sample inlet of a gas chromatograph, and setting the temperature of a column box: slowly heating from room temperature to 80 ℃ at the heating rate of 5K/min, preserving heat, aging for 8h, cooling to the sample measuring temperature, and connecting the opening of the second packed column with a detector;
s2: after the observation of the stable baseline, setting the sample introduction temperature of 100 ℃ and the column temperature box: constant temperature of 30 ℃, carrier gas: helium, carrier gas pressure: 0.1MPa, carrier gas flow rate: 20ml/min, detector temperature: the gas sample amount is not more than 2ml and the liquid sample amount is not more than 0.5 mul at 80 ℃.
To further illustrate the embodiments of the present invention in detail, the following description will be given by referring to specific examples.
Example 1Preparative gas chromatography column
Respectively purchasing a stainless steel column tube with the outer diameter of 3mm, the inner diameter of 1.5mm and the length of 5m and a PTFE column tube with the outer diameter of 3mm, the inner diameter of 1.5mm and the length of 3m, sequentially cleaning the column tubes by using 5% hot KOH solution and 3% HCl solution, continuously washing by using 500ml deionized water, and then drying the column for later use;
taking the specific surface area of more than or equal to 250m2Treating the microsphere silica gel per gram in an oven at 200 ℃ for 24 hours, drying the PTFE micropowder for 10 minutes under an infrared lamp, respectively weighing 17.7ml of microsphere silica gel and 13.9ml of PTFE micropowder in A, B two beakers, and weighing the beakers respectively to be 10.34g and 10.85 g; respectively weighing 1.14g and 2.38g of polytrifluorochloroethylene oil in C, D beakers, respectively adding 20ml of acetone, stirring until the mixture is completely dissolved, adding microsphere silica gel in the beaker A into a beaker C containing a completely dissolved stationary liquid solution while stirring, placing the beaker D into an ultrasonic cleaner, setting the ultrasonic power to be 100W, adding PTFE micro powder in the beaker B into the completely dissolved stationary liquid solution while stirring, and performing ultrasonic treatment until no bubbles exist; placing C, D two beakers under an infrared lamp until the solvent is completely evaporated, and sieving the filler D under the infrared lamp by a 100-mesh sieve to ensure that the filler is dry and free of agglomeration;
and (3) completely filling the carrier in the step C into a stainless steel column with the diameter of 5m by using a decompression method, completely filling the carrier in the step D into a PTFE column with the diameter of 3m, continuously tapping the filling column to uniformly distribute the carrier in the filling process, observing whether the carrier in the PTFE column tube is tightly filled under light, plugging the column head by using glass wool after filling, placing a stainless steel liner tube with the diameter of 1.5mm into the PTFE column head, and connecting the two chromatographic columns in series by using stainless steel nuts.
The stainless steel column tube is purchased from ATEO company, the PTFE column tube is produced and sold by Zhonghao Chen optical chemical research institute Co., Ltd, and the microsphere silica gel, the PTFE micropowder and the polytrifluorochloroethylene oil are purchased from Lanzhou Dongliong Co., Ltd.
Example 2
The application effect of the gas chromatography column was verified by separating a sample containing a low-boiling fluorine-containing compound with the gas chromatography column prepared in example 1.
Evaluation was performed using an SC-3000 gas chromatograph (chongqingchuan instrument, TCD detector) and a chromatographic workstation N6000 (intelligent information engineering institute of zhejiang university).
The experimental parameters were as follows:
temperature of the gasification chamber: 80 ℃;
column oven: keeping the temperature constant at 30 ℃;
carrier gas: helium gas;
carrier gas pressure: 0.1 MPa;
flow rate of carrier gas: 20 ml/min;
detector temperature: 80 ℃;
polarity: positive;
bridge flow: 150 mA;
taking 1ml of mixed gas for sample injection, wherein the mixed gas comprises the following known components: c2F4、F2、CF4、CF3OF、COF2、CF3COF, determining the attribution of chromatographic peak components by an internal standard method, wherein the evaluation result is shown in Table 1, and the obtained gas chromatogram is shown in FIG. 1.
TABLE 1
| Retention time | Concentration of | Peak area | Peak height | Components |
| 1.894 | 3.13 | 309395 | 40787 | F2 |
| 2.367 | 2.01 | 198408 | 24352 | CF4 |
| 3.100 | 80.37 | 7950318 | 576284 | CF3OF |
| 4.242 | 1.99 | 197742 | 9427 | COF2 |
| 5.134 | 7.66 | 758374 | 22131 | C2F4 |
| 7.697 | 4.84 | 478029 | 20325 | CF3COF |
From the data in table 1 and with reference to fig. 1, it can be seen that the chromatographic column has excellent separation efficiency, rapid separation, standard and beautiful peak shape, and can completely separate the above 6 compounds. According to the quantitative results in Table 1, the component content can be accurate to 2 bits after decimal point.
Experiments show that the gas chromatographic column provided by the embodiment 1 of the invention is applied to the analysis of low-boiling-point fluorine-containing compounds, and the service life is more than 5000 h.
Comparative example 1
The sample containing the low boiling point fluorine-containing compound was separated by a conventional polar column, and the sample was the same as that of example 2. The used polar chromatographic column adopts a stainless steel column tube, the outer diameter of the column tube is 3mm, the inner diameter of the column tube is 1.5mm, the length of the column tube is 15m, the carrier selects microsphere silica gel of 80-100 meshes, and the stationary liquid is 25% of middle phenyl polysiloxane.
Evaluation was also carried out using an SC-3000 gas chromatograph (chongqing instrument, TCD detector), a chromatographic workstation N6000 (intelligent information engineering institute of zhejiang university).
The experimental parameters were as follows:
temperature of the gasification chamber: 120 ℃;
column oven: keeping the temperature at 70 ℃;
carrier gas: helium gas;
carrier gas pressure: 0.05 MPa;
flow rate of carrier gas: 10 ml/min;
detector temperature: 100 ℃;
polarity: positive;
bridge flow: 150 mA;
taking 1ml of mixed gas for sample injection, wherein the mixed gas comprises the following known components: c2F4、F2、CF4、CF3OF、COF2、CF3COF, determining the attribution of chromatographic peak components by an internal standard method, wherein the evaluation result is shown in Table 2, and the obtained gas chromatogram is shown in FIG. 2.
TABLE 2
| Retention time | Concentration of | Peak area | Peak height | Components |
| 14.276 | 3.46 | 841359 | 9515 | F2 |
| 16.474 | 2.21 | 535538 | 9832 | CF4 |
| 23.548 | 94.33 | 22884669 | 127581 | Mixed gas (es) |
From the data in Table 2, in conjunction with FIG. 2, it can be seen that the conventional polar chromatography column has a long separation time, F2And CF4Poor chromatographic peak shape, C2F4、CF3OF、COF2、CF3COF and other 4 kinds of gases only react to form one chromatographic peak, and the fluorine-containing compound is not availableEffective separation is achieved. And the service life of the polar chromatographic column applied to the analysis of the fluorine-containing mixed gas provided by the prior art is not more than 100 h.
Compared with a comparative example, the gas chromatographic column provided by the invention is obviously superior to the existing chromatographic column, and is beneficial to realizing the quantitative analysis of the low-boiling-point fluorine-containing compound.
The gas chromatographic column provided by the invention has stable performance, can realize good chromatographic separation efficiency at room temperature, can protect the carrier from being oxidized, and greatly prolongs the service time of the chromatographic column. The preparation method of the chromatographic column is simple, convenient to use and good in reproducibility.
Claims (10)
1. The utility model provides a gas chromatography column, its characterized in that, is including the first packed column and the second packed column that concatenate, pack the microballon silica gel carrier of coating polytrifluorochloroethylene in the first packed column, pack the PTFE miropowder carrier of coating polytrifluorochloroethylene in the second packed column.
2. The gas chromatographic column as claimed in claim 1, wherein the microsphere silica gel carrier coated with polychlorotrifluoroethylene is prepared by impregnating the microsphere silica gel carrier with polychlorotrifluoroethylene oil, and the mass ratio of the microsphere silica gel carrier to the polychlorotrifluoroethylene oil is (8-10) to 1.
3. The gas chromatographic column as claimed in claim 1, wherein the PTFE micro powder carrier coated with the polychlorotrifluoroethylene is prepared by impregnating and coating a PTFE micro powder carrier with polychlorotrifluoroethylene oil, and the mass ratio of the PTFE micro powder carrier to the polychlorotrifluoroethylene oil is (4-6) to 1.
4. The gas chromatography column of claim 2 or 3, wherein the microspherical silica gel support has a particle size of 80-100 mesh and/or a specific surface area of not less than 250m2(ii)/g; the particle size of the PTFE micro powder carrier is 80-100 meshes.
5. The gas chromatography column of claim 4, wherein the first packed column and the second packed column have a column length ratio of (4-6) to 3.
6. The gas chromatography column of claim 5, wherein the first packed column is a stainless steel column and the second packed column is a PTFE column.
7. The gas chromatography column of claim 6, wherein the first packed column has a column length of 5m and the second packed column has a column length of 3 m; the inner diameters of the first packed column and the second packed column are both 1.5 mm.
8. Use of a gas chromatography column as claimed in any of claims 1 to 7 for separating and/or analyzing samples containing low boiling point fluorine-containing compounds, optionally selected from C2F4、F2、CF4、CF3OF、COF2And CF3One or more of COFs.
9. The use of claim 8, wherein the opening of the first packed column is a sample inlet port for connection with a gas chromatograph sample inlet port, and the opening of the second packed column is a detector port for connection with a detector.
10. A method for separating low boiling fluorine-containing compounds using the gas chromatography column of any one of claims 1 to 7, comprising the steps of:
(1) connecting an opening of the first packed column with a sample inlet of a gas chromatograph, and connecting an opening of the second packed column with a detector; helium is used as carrier gas, the pressure of the carrier gas is 0.05-0.15 MPa, the flow rate of the carrier gas is set to be 20-30 ml/min, the temperature of a column box is increased from room temperature to 75-85 ℃ at the temperature increase rate of 4-6K/min, the temperature is kept, the aging is carried out, and then the temperature is reduced to the sample measuring temperature;
(2) after the observation base line is stable, the sample injection temperature is set to 95-105 ℃, the column oven is set to be constant at 25-35 ℃, and the detector temperature is set to 75 ∞Sampling a sample to be detected at 85 ℃, and performing separation detection; the sample to be detected is a sample containing the low-boiling-point fluorine-containing compound, and the low-boiling-point fluorine-containing compound is optionally selected from C2F4、F2、CF4、CF3OF、COF2And CF3One or more of COFs.
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| CN115372532A (en) * | 2022-07-29 | 2022-11-22 | 广西电网有限责任公司电力科学研究院 | Packing chromatographic column for analyzing sulfur hexafluoride decomposition product and preparation method |
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